Classifications

• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B33/00—Silicon; Compounds thereof
  • C01B33/20—Silicates
  • C01B33/32—Alkali metal silicates
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/02—Inorganic compounds ; Elemental compounds
  • C11D3/12—Water-insoluble compounds
  • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
  • C11D3/1246—Silicates, e.g. diatomaceous earth
  • C11D3/1253—Layer silicates, e.g. talcum, kaolin, clay, bentonite, smectite, montmorillonite, hectorite or attapulgite
  • C11D3/1273—Crystalline layered silicates of type NaMeSixO2x+1YH2O

Definitions

• the invention relates to a sparingly soluble alkali metal silicate, to a process for its preparation and to its use in detergents and cleaners.
• Crystalline sheet sodium silicates (phyllosilicates) of the formula NaMSi x O 2x+1 .yH 2 O, where M is sodium or hydrogen, x is a number from 1.9 to 4 and y is a number from 0 to 20, and preferred values for x are 2, 3 or 4, have proven to be suitable replacements for the detergent builders phosphate and zeolite.
• M sodium or hydrogen
• x is a number from 1.9 to 4
• y is a number from 0 to 20
• preferred values for x are 2, 3 or 4
• the use of such crystalline phyllosilicates for softening water is described, for example, in EP-A-0 164 514.
• Detergent builders fulfill a large number of functions. Of these, particular mention may be made of the removal of or reduction in water hardness in the mains water used for washing and the supply of alkalinity, i.e. the regulation of and increase in the pH in the wash liquor.
• the abovementioned inorganic incrustations consist of water hardness precipitated out in the form of calcium carbonate or of deposited residues of dissolved detergent builder components.
• the desired increase in the pH in the wash liquor results in the soil particles which may be present having a higher surface charge, making them easier to remove from the fabric being washed.
• Silicatic detergent builders are divided into readily soluble types and sparingly soluble types.
• Readily soluble silicatic detergent builders are frequently pure X-ray-amorphous sodium silicates. Although these sodium silicates, which are prepared from spray-dried sodium water glass, are able to contribute to the regulation of the pH, they are only able to make a small contribution to the lowering of the water hardness.
• Sparingly soluble detergent builders which primarily include the aluminum-containing silicates (zeolites), are, however, not able by themselves to favorably influence the pH in the wash solution, i.e. to provide higher alkalinity of the wash solution.
• zeolites aluminum-containing silicates
• the object of the present invention was therefore to provide a sparingly soluble builder based on alkali metal silicate which has both a high water-softening capacity and is itself highly effective as a builder.
• a sparingly soluble alkali metal silicate of the type mentioned in the introduction which comprises alkali metal phyllosilicates in finely divided form in a non-phyllosilicatic alkali metal silicate environment of the formula x M I 2 O.y SiO 2 , in which M I is an alkali metal and y/x is (1.9 to 500): 1.
• M I is an alkali metal
• y/x is (1.9 to 500): 1.
• the crystalline alkali metal silicate preferably corresponds overall to the formula
• M I is an alkali metal
• M II is an alkaline earth metal
• X is an element of the third main group
• Z is an element of the fifth main group of the Periodic Table of the Elements and the following also applies:
• y/x is (2.0 to 200): 1.
• M I is preferably sodium.
• the non-phyllosilicatic alkali metal silicate environment is preferably composed of non-phyllosilicatic sodium silicate.
• non-phyllosilicatic sodium silicates include, in particular, the amorphous sodium silicates which, in the X-ray powder diffractogram, typically exhibit no sharp reflections which can be assigned to an ordered crystalline structure; they do not have a defined stoichiometric composition either.
• the alkali metal phyllosilicate is preferably composed of sheet crystalline disodium disilicates.
• the latter in turn usually consist of at least one polymorphous phase.
• the sparingly soluble alkali metal silicate preferably consists of
• beta-disodium disilicate 0 to 60% by weight of beta-disodium disilicate
• the sparingly soluble alkali metal silicate consists of
• the sparingly soluble alkali metal silicate consists of
• beta-disodium disilicate 0 to 40% by weight of beta-disodium disilicate
• the sparingly soluble alkali metal silicate consists of
• beta-disodium disilicate 0 to 40% by weight of beta-disodium disilicate
• the sparingly soluble alkali metal silicate consists of
• beta-disodium disilicate 0 to 50% by weight of beta-disodium disilicate
• the sparingly soluble alkali metal silicate consists of
• the sparingly soluble alkali metal silicate consists of
• beta-disodium disilicate 0 to 10% by weight of beta-disodium disilicate
• the sparingly soluble alkali metal silicate preferably comprises up to 10% by weight, based on the alkali metal silicate content, of further constituents.
• the further constituents are preferably cationic and/or anionic constituents.
• the cationic constituents are preferably alkali metal ions and/or alkaline earth metal cations and/or Fe, W, Mo, Ta, Pb, Sn, Al, Zn, Ti, V, Cr, Mn, Co and/or Ni.
• the anionic constituents are preferably sulfates, fluorides, chlorides, bromides, iodides, carbonates, hydrogencarbonates, nitrates, oxide hydrates, phosphates and/or borates.
• the sparingly soluble alkali metal silicate preferably comprises up to 10 mol% of boron, based on the total content of SiO 2 .
• the sparingly soluble alkali metal silicate preferably comprises up to 50 mol% of phosphorus, based on the total content of SiO 2 .
• the sparingly soluble alkali metal silicate preferably has, as powder, a mean particle diameter of from 0.1 to 150 ⁇ m.
• the sparingly soluble alkali metal silicate preferably has, as compacted granulate, a mean particle diameter of from 10 to 2000 ⁇ m.
• the present object is likewise achieved by a process for the preparation of sparingly soluble alkali metal silicates, which comprises mixing a sodium silicate-containing starting material with one or more compounds which comprise the components M I , M II , X and/or Z, and crystallizing the mixture.
• M I is an alkali metal
• M II is an alkaline earth metal
• X is an element of the third main group
• Z is an element of the fifth main group of the Periodic Table of the Elements.
• Suitable compounds are preferably the oxides, although other compounds are also suitable.
• the mixing ratio of the reactants is preferably chosen such that the mixture has a composition which corresponds to the composition of the above-described alkali metal silicates according to the invention.
• the sodium silicate-containing starting material used is preferably water glass.
• water glass is mixed with sodium hydroxide solution, water glass or other silicate sources, spray-dried and crystallized.
• the crystallization temperature is preferably 700 to 1300 K.
• the crystallization temperature is preferably 800 to 1200 K.
• the crystallization temperature is particularly preferably 900 to 1100 K.
• the invention also relates to the use of sparingly soluble alkali metal silicate for the preparation of detergents and cleaners, including dishwashing detergents.
• the invention likewise relates to detergents and cleaners which comprise a sparingly soluble alkali metal silicate according to the invention.
• the detergents and cleaners preferably comprise
• the detergents and cleaners preferably comprise
• the detergents and cleaners preferably comprise
• the detergents and cleaners preferably comprise
• the detergents and cleaners preferably comprise
• the detergents and cleaners preferably comprise
• the detergents and cleaners preferably comprise
• the detergents and cleaners preferably comprise
• the detergents and cleaners preferably comprise
• the detergents and cleaners preferably comprise
• the preferred range in the abovementioned detergents and cleaners for the sparingly soluble alkali metal silicate is between 1 and 50% by weight and particularly preferably between 3 and 30% by weight. According to other embodiments of the invention, contents of from 60 to 98% by weight and particularly from 70 to 98% by weight are preferred.
• detergents and cleaners are, for the cobuilders, 1 to 50% by weight and 1 to 30% by weight; for the pH regulators, likewise 1 to 50% by weight and 1 to 30% by weight, for the surface-active substances 1 to 30% by weight and 1 to 20% by weight and for the bleaching system 1 to 40% by weight and 1 to 20% by weight.
• the cobuilders are preferably crystalline aluminosilicates, mono-, oligo- or polymeric carboxylic acids, alkali metal carbonates, alkali metal ortho-, pyro-, polyphosphates, crystalline alkali metal silicates having a crystal lattice without a sheet structure and/or amorphous alkali metal silicates.
• the bleaching system is preferably an active chlorine and/or active oxygen carrier, bleach activator, bleach catalyst, enzymes used to remove diskolorations, perborate and/or percarbonate.
• the surface-active substances are preferably anionic, cationic, nonionic and/or zwitterionic surfactants.
• the pH regulators are preferably soda, citric acid, sodium citrate and/or bicarbonate.
• the reaction with sand can be carried out hydrothermally, i.e. in aqueous solution at elevated pressure and temperature or thermally (tank furnace) by melting or heat-treating the reactants with one another.
• a molar ratio of SiO 2 to Na 2 O of 1.9 ⁇ e ⁇ 4 is set in the abovementioned water glass, and then the starting material obtained in this way is treated with heat.
• the starting material can also be modified prior to heat treatment:
• One embodiment involves converting the solution produced in the hydrothermal process to the solid form and/or changing the water content of the solid form.
• the water content can be increased by spraying with water (e.g. in a Lödige, Telschig or Schugi mixer), or lowered by afterdrying (e.g. belt, fluidized-bed, flotation dryer).
• a further embodiment involves converting the solid produced during the thermal process to the liquid form and/or optimally adjusting the water content in the liquid solution by evaporation or dilution.
• the redrying of the solution to give a spray-dried alkali metal silicate is preferred.
• a further embodiment involves admixing the solid produced during the thermal process with water and subjecting it to heat treatment.
• the heat treatment is decisive.
• material temperatures of from 700 K to 1300 K are suitable. Preference is given to temperatures of from 800 K to 1200 K. Particular preference is given to temperatures of from 900 K to 1100 K.
• the temperature can be distributed evenly within the furnace.
• Preferred apparatuses which are used are rotary tubes, fluidized bed furnaces, ingot molding furnaces, belt furnaces, entrained-dust furnaces, muffle furnaces.
• the heat can be introduced into the material directly, indirectly, by convection, radiation heating or contact heating.
• the further constituents can be added at any desired stage before or after crystallization. It is preferred to add the further constituents to the reaction with the sand. It is particularly preferred to meter the further constituents into the solution from the reaction with the sand. It is likewise preferred to meter in the further constituents in the course of the atomization of the solution during the spray drying to just such a solution.
• the product can preferably be changed physically.
• the particle size is optimally adjusted by grinding and subsequent classification. Suitable for the grinding are, for example, vibratory mills, ball mills, roller mills and pendulum roller mills from Neuman & Esser, and airjet mills, such as the models from Hosokawa-Alpine. Sifting and/or screening are used for the classification. For the screening, Aligaier, Rhewum and Locker screens, for example, can be used.
• the ground powder is admixed with a granulation auxiliary on a pelletizing disk or a mixer.
• a granulation auxiliary on a pelletizing disk or a mixer.
• shear forces the material agglomerates.
• One embodiment involves subsequently drying the material.
• a further embodiment involves leaving the material undried.
• Granulation auxiliaries may be: bentonites, hectorites, saponites, modified or unmodified celluloses, polymers and copolymers, water glass, surfactants and other detergent ingredients.
• the particle size is preferably optimally adjusted by roll compaction, grinding and subsequent classification.
• the ground powder is optionally mixed with an auxiliary and compacted in a roll compactor (Hosokawa-Bepex, Alexanderwerk).
• the compaction pressure is between 2 and 100 kN/cm 2 roller width. Where appropriate, the material can be subsequently dried.
• Compaction auxiliaries may be: bentonites, hectorites, saponites, modified or unmodified celluloses, polymers and copolymers, water glass, surfactants and other detergent ingredients.
• the particularly fine distribution can be achieved according to the invention by adjusting the M I 2 O/SiO 2 ratio of the material in the starting material, and then crystallizing the alkali metal phyllosilicates, preference being given here to sodium phyllosilicates.
• the further constituents are preferably not in the phyllosilicatic fraction, but in the nonsilicatic fraction.
• the phyllosilicatic fractions can also have considerable amounts of other constituents.
• the sparingly soluble alkali metal silicates according to the invention can, as stated above, be used in detergents and cleaners. Preference is given here to pulverulent heavy-duty, color and specialty detergents. Heavy-use detergents are balanced formulations with the aim of as high a detergency as possible. Color detergents are intended primarily to protect colored textiles with regard to bleaching and fading of the colors and felting of the fibers. Specialty detergents are aimed at narrow areas of application, such as stain-removal salts, bleach boosters, curtain detergents, wool detergents etc.
• Builder silicates can also be used in water softeners, which, primarily in regions of high water hardness, have a performance-enhancing effect on the wash result and a protective effect with regard to the washing machine.
• Silicates are required here primarily because of their good soil dispersion, their high alkalinity and because of their protective action against damage to glassware. Glass damage here means the formation of layered deposits on glassware or the erosion of the glass surface. Both lead to the known undesired hazing of glassware.
• Detergents and cleaners in their form as detergents, water softeners and machine dishwashing detergents can be used in powder form, granulate form and tablet form.
• the detergent formulation is mixed and compressed to the appropriate shape using a tableting press.
• the shape can be cylindrical or cuboid or optionally also assume largely any desired other geometric shapes.
• the radius to height ratio can be between 0.25 and 4.
• the compaction pressure can be between 12 and 0.3 kN/cm 2 . This is essentially independent of the geometric shape of the tablet. Preference is also given to multistage compression. For this, any desired components of the formulation are compressed consecutively on one another in a plurality of stages, resulting in a plurality of layers. In the case of a two-layer tablet, a volume ratio of the two layers of from 1:10 to 10:1 is particularly preferred.
• the size of particles in aqueous dispersion is determined using an ASVR/FRA Microtrac granulometer from Leeds & Northrup.
• the parameter measured is the reflection or diffraction of a laser beam upon passing through the dispersion. 400 ml of ethanol are pumped through the laser measurement cell.
• the solid sample e.g. 70 mg
• the evaluation unit of the instrument calculates the mean particle diameter (d 50 value).
• the inserts having the desired screens are inserted into a Retsch screening machine.
• the mesh width of the screens decreases from top to bottom.
• 50 g of the sample material to be investigated are placed on the widest screen.
• the residues on the screens are weighed and calculated on the basis of the initial weight of material.
• the d 50 value can be calculated from the results.
• a mixture of a buffer stock solution and deionized water is introduced into a ErWeKa dissolution tester, stirred and heat-treated at 30° C.
• the buffer stock solution is an aqueous solution of glycine, sodium chloride, calcium chloride and sodium hydroxide in suitable concentrations.
• the calcium-sensitive electrode Model 932001 from Orion is dipped into the solution and calibrated by replenishing the solution with a calcium stock solution. This is carried out using the EA 940 evaluation unit from Orion. After replenishing, the solution has a water hardness of 17 degrees German water hardness.
• the Orion EA 940 is started.
• the pH of the measurement solution is 10.2.
• the Orion EA 940 gives the concentration of free calcium ions at specific time intervals. Using the previously determined initial weight of calcium, the concentration of free, unbonded calcium ions after 10 min is used to deduce the amount of bonded calcium, i.e. the calcium-binding capacity. This is given in mg of CaCO 3 /g.
• a sample of 1.3 g of the material under investigation is added to about 100 ml of demineralized water and completely dissolved by stirring for 30 minutes at 50° C.
• the amount of SiO 2 and Na 2 O is then determined in each case by titration, and the SiO 2 :Na 2 O ratio is calculated by calculating their molar amounts and relating them to one another.
• a sample of the material under investigation is pulverized in a mortar and measured in a Philips PW1710 X-ray powder diffractometer (Parameter: Cu K alpha 2 radiation, wavelength 1.54439 Angström, accelerating potential 35kV, heating current 28 mA, monochromator, scanning rate 3 degrees 2 theta per minute).
• the resulting intensities are evaluated as follows.
• Beta phase 2.97+/ ⁇ 0.06 SKS-7 (EP 0 164 552)
• the JCPDS numbers refer to the reference diffractograms of substances listed by the Joint Committee of Powder Diffraction Standards.
• the contents of the alpha, beta, delta phases of the silicates are calculated in percent from the intensities I a , I b , I d —measured in pulses—of the alpha, beta, delta phases in accordance with the following formulae:
• non-phyllosilicatic sodium silicate [AM] the background (pulse) of the X-ray peak is determined at a d value of 2.65 Angström (I am ) and converted to the percentage content using the following empirical formula.
• a roll compactor In a roll compactor (Hosokawa-Bepex, model: L200/50P), the material to be compacted is conveyed between the compactor rollers using a stuffing screw (setting: stage 5). This is done at such a rate that a nip length of 50 mm produces a compaction pressure of from 140 to 160 kN.
• the roller rotation is set at stage 3 to 7, and the roller gap is 0.1 mm.
• the resulting sticks (length: about 50 mm, thickness: about 2 to 5 mm, width about 10 to 15 mm) are crushed in a hammer mill (Alpine, model UPZ) having a perforation diameter of 5 mm at a rotary speed of from 600 to 1400 rpm. From the crushed pulverulent product are removed oversize particles (using a screen with a perforation diameter of 1.4 mm) and undersize particles (perforation diameter 0.25 mm).
• the optical brighteners are stirred into a quarter of the amount of alkyl ethoxylate (AE) and mixed in a domestic multimixer (Braun) with half of the amount of soda.
• AE alkyl ethoxylate
• Braun domestic multimixer
• the remaining soda and all of the zeolite and polymer are mixed at 300 rpm for 15 minutes.
• half of the remaining nonionic is sprayed on over the course of 5 minutes.
• the sparingly soluble alkali metal silicate according to the invention is then added and mixed for 10 minutes.
• the remaining second half of the AE is then sprayed on over the course of a further 5 minutes.
• LAS, soap, antifoam, phosphonate and compounds with optical brightener are added and subsequently mixed at 300 rpm for 10 minutes.
• a tumble mixer the mixture from the Lödige mixer is admixed, with low shear stress, with perborate, TAED and enzymes, and mixed for 15 minutes.
• test fabrics were washed at 60° C. and a water hardness of 18° German hardness with a test detergent at a dosing of 65 or 135 g/wash cycle.
• the test fabrics were supplemented with further laundry ballast (3.75 kg).
• test fabrics which are a cotton terry fabric (Vossen), in each case a cotton double-rib fabric, polyester/cotton blend (type 20A) and standard cotton fabric (type 10A) from Waschereiutz Testgewebe GmbH and a standard cotton fabric from the Swiss Materials Testing Institute, St. Gallen, Switzerland were repeatedly washed (15 times) in accordance with the above procedure. After 15 washes, a sample was taken from each of the fabrics and ashed in a muffle furnace at a temperature of 1000° C. for a period of 24 hours. The weights of the residues are calculated based on the amounts of fabric (weights) used.
• a test ultracompact heavy-duty detergent comprising 30.0% of commercially available zeolite was prepared in accordance with the general procedure “Preparation of the test detergents”. The procedure was adapted inasmuch as the optical brighteners are stirred in a quarter of the alkyl ethoxylate (AE) and mixed with a third of the amount of soda. The remaining soda, the polymer and all of the zeolite are mixed in the Lödige mixer, and the remaining AE is sprayed on. Then, all of the other components with the exception of enzymes, TAED and perborate are mixed in. The latter are then mixed into the mixture prepared in the Lödige mixer in a tumble mixer.
• AE alkyl ethoxylate
• inorganic incrustations and the detergency were investigated in model washing experiments in accordance with the general procedures “Washing experiments”, “Determination of the inorganic incrustation” and “Determination of the detergency”: inorganic incrustation 3.30%, detergency 15.9%.
• a test ultracompact heavy-duty detergent comprising 10.0% of the silicate from Example 1 was prepared in accordance with the general procedure “Preparation of the test detergents”. The procedure was adapted inasmuch as the remaining soda, the polymer and all of the zeolite are mixed in a Lödige mixer, then half of the remaining AE is sprayed on, then the silicate from Example 1 is mixed in and finally the remaining AE is sprayed on. All of the other components with the exception of enzymes, TAED and perborate are then mixed in. The latter are then mixed into the mixture prepared in the Lödige mixer in a tumble mixer.
• inorganic incrustations and the detergency were investigated in model washing experiments in accordance with the general procedures “Washing experiments”, “Determination of the inorganic incrustation” and “Determination of the detergency”: inorganic incrustation 2.54%, detergency 18.1%.
• a test ultracompact heavy-duty detergent comprising 10.0% of the silicate from Example 4 was prepared in accordance with the general procedure “Preparation of the test detergents”. The procedure was adapted inasmuch as the remaining soda, the polymer and all of the zeolite are mixed in a Lödige mixer, then half of the remaining AE is sprayed on, then the silicate from Example 4 is mixed in and finally the remaining AE is sprayed on. All of the other components with the exception of enzymes, TAED and perborate are then mixed in. The latter are then mixed into the mixture prepared in the Lödige mixer in a tumble mixer.
• inorganic incrustations and the detergency were investigated in model washing experiments in accordance with the general procedures “Washing experiments”, “Determination of the inorganic incrustation” and “Determination of the detergency”: inorganic incrustation 2.41%, detergency 17.7%.
• a test ultracompact heavy-duty detergent comprising 10.0% of the silicate from Example 7 was prepared in accordance with the general procedure “Preparation of the test detergents”. The procedure was adapted inasmuch as the remaining soda, the polymer and all of the zeolite are mixed in a Lbdige mixer, then half of the remaining AE is sprayed on, then the silicate from Example 7 is mixed in and finally the remaining AE is sprayed on. All of the other components with the exception of enzymes, TAED and perborate are then mixed in. The latter are then mixed into the mixture prepared in the Lödige mixer in a tumble mixer.
• inorganic incrustations and the detergency were investigated in model washing experiments in accordance with the general procedures “Washing experiments”, “Determination of the inorganic incrustation” and “Determination of the detergency”: inorganic incrustation 1.97%, detergency 18.2%.
• a test ultracompact heavy-duty detergent comprising 10.0% of the silicate from Example 8 was prepared in accordance with the general procedure “Preparation of the test detergents”. The procedure was adapted inasmuch as the remaining soda, the polymer and all of the zeolite are mixed in a Lödige mixer, then half of the remaining AE is sprayed on, then the silicate from Example 8 is mixed in and finally the remaining AE is sprayed on. All of the other components with the exception of enzymes, TAED and perborate are then mixed in. The latter are then mixed into the mixture prepared in the Lödige mixer in a tumble mixer.
• inorganic incrustations and the detergency were investigated in model washing experiments in accordance with the general procedures “Washing experiments”, “Determination of the inorganic incrustation” and “Determination of the detergency”: inorganic incrustation 1.63%, detergency 18.5%.
• a test ultracompact heavy-duty detergent comprising 10.0% of the silicate from Example 9 was prepared in accordance with the general procedure “Preparation of the test detergents”. The procedure was adapted inasmuch as the remaining soda, the polymer and all of the zeolite are mixed in a Lödige mixer, then half of the remaining AE is sprayed on, then the silicate from Example 9 is mixed in and finally the remaining AE is sprayed on. All of the other components with the exception of enzymes, TAED and perborate are then mixed in. The latter are then mixed into the mixture prepared in the Lödige mixer in a tumble mixer.
• inorganic incrustations and the detergency were investigated in model washing experiments in accordance with the general procedures “Washing experiments”, “Determination of the inorganic incrustation” and “Determination of the detergency”: inorganic incrustation 1.77%, detergency 18.9%.
• a test ultracompact heavy-duty detergent comprising 30.0% of the silicate from Example 9 was prepared in accordance with the general procedure “Preparation of the test detergents”. The procedure was adapted inasmuch as the optical brighteners are stirred in a quarter of the alkyl ethoxylate (AE) and mixed with a third of the amount of sulfate. The remaining sulfate and the total amount of the silicate from Example 9 are mixed in a Lödige mixer, and the remaining AE is sprayed on. All of the other components apart from enzymes, TAED and percarbonate are then mixed in. The latter are then mixed into the mixture prepared in the Lödige mixer in a tumble mixer.
• AE alkyl ethoxylate
• inorganic incrustations and the detergency were investigated in model washing experiments in accordance with the general procedures “Washing experiments”, “Determination of the inorganic incrustation” and “Determination of the detergency”: inorganic incrustation 2.40%, detergency 21.0%.
• a test ultracompact heavy-duty detergent comprising 47% of the silicate from Example 4 was prepared in accordance with the general procedure “Preparation of the test detergents”. The procedure was adapted inasmuch as the optical brighteners are stirred in a quarter of the alkyl ethoxylate (AE) and mixed with two thirds of the amount of bicarbonate. The remaining bicarbonate and the total amount of the silicate from Example 4 are mixed in a Lödige mixer, and the remaining AE is sprayed on. All of the other components apart from enzymes, TAED and percarbonate are then mixed in. The latter are then mixed into the mixture prepared in the Lödige mixer in a tumble mixer.
• AE alkyl ethoxylate
• inorganic incrustations and the detergency were investigated in model washing experiments in accordance with the general procedures “Washing experiments”, “Determination of the inorganic incrustation” and “Determination of the detergency”: inorganic incrustation 2.13%, detergency 23.2%.
• a test standard heavy-duty detergent comprising 10% of the silicate from Example 7 was prepared in accordance with the general procedure “Preparation of the test detergents”. The procedure was adapted inasmuch as the optical brighteners are stirred into the total amount of the alkyl ethoxylate (AE) and mixed with a third of the amount of sulfate. The remaining sulfate, the phosphate, and the total amount of the silicate from Example 7 are mixed in a Lödige mixer. All of the other components apart from enzymes and percarbonate are then mixed in. The latter are then mixed into the mixture prepared in the Lödige mixer in a tumble mixer.
• AE alkyl ethoxylate
• inorganic incrustations and the detergency were investigated in model washing experiments in accordance with the general procedures “Washing experiments”, “Determination of the inorganic incrustation” and “Determination of the detergency”: inorganic incrustation 2.10%, detergency 17.5%.
• a test standard heavy-duty detergent comprising 4% of the silicate from Example 8 was prepared in accordance with the general procedure “Preparation of the test detergents”. The procedure was adapted inasmuch as the optical brighteners are stirred into half of the alkyl ethoxylate (AE) and mixed with two thirds of the amount of sulfate. The remaining sulfate, the soda, the polymer, all of the zeolite and the silicate from Example 8 are mixed in a Lödige mixer, then the remaining AE is sprayed on. All of the other components apart from enzymes, TAED and perborate are then mixed in. The latter are then mixed into the mixture prepared in the Lbdige mixer in a tumble mixer.
• AE alkyl ethoxylate
• inorganic incrustations and the detergency were investigated in model washing experiments in accordance with the general procedures “Washing experiments”, “Determination of the inorganic incrustation” and “Determination of the detergency”: inorganic incrustation 2.34%, detergency 16.9%.
• a test standard heavy-duty detergent comprising 10% of the silicate from Example 9 was prepared in accordance with the general procedure “Preparation of the test detergents”. The procedure was adapted inasmuch as all of the zeolite, the polymer and the bicarbonate are mixed in a Lödige mixer, then the first half of the AE is sprayed on, and then the silicate from Example 9 and the sulfate are mixed in, and finally the remaining AE is sprayed on. All of the other components apart from the enzymes are then mixed in. The latter are then mixed into the mixture prepared in the Lödige mixer in a tumble mixer.
• inorganic incrustations and the detergency were investigated in model washing experiments in accordance with the general procedures “Washing experiments”, “Determination of the inorganic incrustation” and “Determination of the detergency”: inorganic incrustation 1.80%, detergency 17.6%.
• a test water softener comprising 15% of the silicate from Example 8 was prepared in accordance with the general procedure “Preparation of the test detergents”. The procedure was adapted inasmuch as all of the zeolite, the polymer, the bicarbonate, the citric acid, the sulfate and the silicate from Example 8 are mixed in a Lödige mixer, and then the AE is sprayed on. The remaining components are then mixed in.
• inorganic incrustations and the detergency were investigated in model washing experiments using a combination of commercially available ultracompact detergent (dosing 55 g, moderate soiling, very low water hardness) and test water softener (dosing 30 g) in accordance with the general procedures “Washing experiments”, “Determination of the inorganic incrustation” and “Determination of the detergency”: inorganic incrustation 1.64%, detergency 16.4%.
• a test ultracompact heavy-duty detergent comprising 15% of the silicate from Example 9 was prepared in accordance with the general procedure “Preparation of the test detergents”. The procedure was adapted inasmuch as the remaining soda, the polymer and all of the zeolite are mixed in a Lödige mixer, then half of the remaining AE is sprayed on, then the silicate from Example 9 is mixed in and finally the remaining AE is sprayed on. All of the other components apart from enzymes, TAED and perborate are then mixed in. The latter are then mixed into the mixture prepared in the Lödige mixer in a tumble mixer.
• Example 24 Detergent tablets were pressed and tested as in Example 24: inorganic incrustation 2.19%, detergency 1 8.1%.
• Machine dishwashing detergents were prepared in accordance with the general procedure “Preparation of the machine dishwashing detergents”.
• a machine dishwashing detergent gel is prepared by mixing water glass, phosphate, soda, sodium hydroxide, phosphonate, polymer, alkanesulfonate, phosphoric ester using a dispergator (Ultraturrax, Hanke und Kunkel). Finally, silicate and sodium hypochlorite are briefly mixed in. Substances used:
• Zeolite A Wessalith P, Degussa Phosphate 1: Sodium tripolyphosphate, e.g. from Thermphos Intl.
• Phosphate 2 Makrophos 1018, BK Giulini Phosphate 3: Thermphos NW coarse Polymer: Sokalan CP5, BASF Soda: Heavy soda, Matthes & Weber Bicarbonate: Solvay Percarbonate: Oxyper C, Solvay Interox Perborate monohydrate Degussa (Perborate mh): Perborate tetrahydrate Degussa (Perborate th): TAED 1: TAED 4049, Clariant TAED 2: TAED 3873, Clariant LAS: Marlon ARL, Hüls AE 1: Genapol OAA 080, Clariant AE 2: Genapol 2822, Clariant Soap: Liga basic soap HM11E Antifoam: 11.Pwd

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• 1999
  • 1999-09-11 DE DE19943551A patent/DE19943551A1/de not_active Withdrawn
• 2000
  • 2000-09-01 EP EP00118945A patent/EP1083148B1/de not_active Expired - Lifetime
  • 2000-09-01 DE DE50014857T patent/DE50014857D1/de not_active Expired - Fee Related
  • 2000-09-08 JP JP2000273703A patent/JP2001115192A/ja not_active Withdrawn
  • 2000-09-09 KR KR1020000053761A patent/KR20010074442A/ko not_active Application Discontinuation
  • 2000-09-11 US US09/659,394 patent/US6743766B1/en not_active Expired - Fee Related

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